CN110726940B - Method for rapidly evaluating cycle performance of high-nickel cathode material of lithium ion battery - Google Patents
Method for rapidly evaluating cycle performance of high-nickel cathode material of lithium ion battery Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 309
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 224
- 238000000034 method Methods 0.000 title claims abstract description 60
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 32
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 239000010406 cathode material Substances 0.000 title claims description 65
- 239000010405 anode material Substances 0.000 claims abstract description 92
- 238000007599 discharging Methods 0.000 claims abstract description 20
- 230000008859 change Effects 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 7
- 238000001514 detection method Methods 0.000 claims abstract description 6
- 239000007774 positive electrode material Substances 0.000 claims description 51
- 238000012360 testing method Methods 0.000 claims description 16
- 230000014759 maintenance of location Effects 0.000 claims description 13
- 230000002427 irreversible effect Effects 0.000 claims description 8
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052744 lithium Inorganic materials 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 238000011156 evaluation Methods 0.000 abstract description 26
- 239000000463 material Substances 0.000 description 13
- 230000008569 process Effects 0.000 description 8
- 230000001133 acceleration Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 230000009466 transformation Effects 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 230000002441 reversible effect Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 229910013716 LiNi Inorganic materials 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003550 marker Substances 0.000 description 2
- 230000036961 partial effect Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 229910018632 Al0.05O2 Inorganic materials 0.000 description 1
- 229910000572 Lithium Nickel Cobalt Manganese Oxide (NCM) Inorganic materials 0.000 description 1
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 description 1
- FBDMTTNVIIVBKI-UHFFFAOYSA-N [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] Chemical compound [O-2].[Mn+2].[Co+2].[Ni+2].[Li+] FBDMTTNVIIVBKI-UHFFFAOYSA-N 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
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- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/382—Arrangements for monitoring battery or accumulator variables, e.g. SoC
- G01R31/3835—Arrangements for monitoring battery or accumulator variables, e.g. SoC involving only voltage measurements
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/36—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC]
- G01R31/378—Arrangements for testing, measuring or monitoring the electrical condition of accumulators or electric batteries, e.g. capacity or state of charge [SoC] specially adapted for the type of battery or accumulator
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Abstract
The invention provides a rapid evaluation method for cycle performance of a high-nickel anode material of a lithium ion battery, which comprises the following steps: providing a high-nickel anode material to be measured and a standard high-nickel anode material meeting the preset cycle performance requirement, and respectively assembling the high-nickel anode material and the standard high-nickel anode material with the same cathode and the same diaphragm into a battery according to the same method to obtain a standard battery and a battery to be measured; performing pre-charging aging and grading treatment on a standard battery and a battery to be detected under the same condition, and charging and discharging for 1-3 cycles at 0.01-1C on a battery detection system; collecting data of charging and discharging capacity (Q) and voltage (V), and drawing dQ/dV-V curves of a standard battery and a battery to be tested; and extracting the peak values H2-H3 with the voltage of 4.0-4.2V according to the dQ/dV-V curve, and judging the cycle performance of the standard battery and the battery to be tested according to the peak values H2-H3 and the change of the peak values.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a rapid evaluation method for cycle performance of a high-nickel anode material of a lithium ion battery.
Background
The lithium ion secondary battery is the most competitive battery of the new generation, is called as green and environment-friendly energy, and is the first choice technology for solving the current environmental pollution problem and energy problem. In recent years, lithium ion secondary batteries have been largely successful in the field of high-energy batteries, but consumers still desire batteries with higher overall performance to come out, depending on research and development of electrode materials and electrolyte systems. The high-nickel cathode material has high nickel content, and nickel is a main oxidation-reduction reaction element, so that the specific capacity of the lithium battery cathode material can be effectively improved.
The current method for evaluating the cycle performance of the high-nickel anode material of the lithium battery mainly comprises the steps of manufacturing a full battery and then testing the cycle life according to a certain cycle standard. Most were fully charged until 80% of the initial life, at which point the test was terminated. Taking a 3C type consumer battery with relatively low requirement on the general service life as an example, the cycle life of 500 times to 1000 times is generally required, and a 1C full-charge discharge system is adopted, and the cycle life of 500 times to 1000 times is about 50 days to 100 days after the test; taking a long-life energy storage battery as an example, the cycle life of 3000 to 6000 times is generally required, and the cycle life of 3000 to 6000 times is about 300 to 600 days after the test by adopting a 1C charging and discharging mode. Obviously, such a long test period not only wastes a lot of time, but also increases a lot of costs including manpower, material resources, and power consumption. The above-described method is still used for the evaluation of the production of a novel positive electrode material.
In view of the above, the conventional method for evaluating the cycle performance of the high nickel positive electrode takes too long, consumes more energy, has too high cost, needs to occupy longer time of the testing equipment, and increases the equipment cost virtually. In the industry, a method for rapidly evaluating the cycle performance of a high-nickel cathode material of a lithium ion battery is urgently needed to be researched.
Disclosure of Invention
The invention aims to provide a method for rapidly evaluating the cycle performance of a high-nickel anode material of a lithium ion battery, and aims to solve the problems of long time consumption, high energy consumption and high cost of the conventional method for evaluating the cycle performance of the high-nickel anode.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a rapid evaluation method for cycle performance of a high-nickel anode material of a lithium ion battery, which comprises the following steps:
providing a high-nickel anode material to be measured and a standard high-nickel anode material meeting the requirement of preset cycle performanceRespectively assembling the standard high-nickel anode material and the high-nickel anode material to be measured with the same cathode and the same diaphragm into a battery according to the same method to obtain a standard battery and a battery to be measured; the Ni content in the high-nickel anode material to be measured and the standard high-nickel anode material is not lower than 80%, and the standard battery is marked as QSThe battery to be tested is QX；
Performing pre-charging aging and capacity grading treatment on the standard battery and the battery to be tested under the same condition, and performing 0.01-1C charging and discharging circulation on the standard battery and the battery to be tested after capacity grading on a battery detection system, wherein the circulation method comprises the following steps:
charging system: charging to 4.2V at constant current and constant pressure of 0.01-0.1 ℃; standing for 1-30 min;
discharge system: 0.01-0.1C, placing the mixture to 2.75V, and standing for 1-30 min;
collecting data of charging and discharging capacity Q and voltage V, and drawing dQ/dV-V curves of a standard battery and a battery to be tested;
extracting H2-H3 peak values with the voltage of 4.0-4.2V according to the dQ/dV-V curve; judging the cycle performance of the standard battery and the battery to be tested according to the H2-H3 peak values and the changes of the standard battery and the battery to be tested; wherein the peak values of the standard battery in the range of 4.0-4.2V from H2-H3 are marked as QS(H2-H3), and the peak values of the to-be-tested battery in the range of 4.0-4.2V, namely H2-H3, are marked as Qx(H2～H3)；
If QX(H2～H3)＞QS(H2-H3), the cycle performance of the high nickel cathode material to be measured is lower than the cycle performance of the standard high nickel cathode material;
if QX(H2～H3)<QS(H2-H3), the cycle performance of the high nickel positive electrode material to be measured is superior to that of the standard high nickel positive electrode material;
if QX(H2～H3)＝QS(H2-H3), and QXThe peak values of H2-H3 are shifted to the right, and the irreversible phase change is increased, so that the cyclicity of the high-nickel anode material to be measured is lower than the cyclicity of the standard high-nickel anode material.
According to the rapid evaluation method for the cycle performance of the high-nickel anode material of the lithium ion battery, provided by the invention, the standard high-nickel anode material meeting the requirement of the preset cycle performance is taken as a reference standard, and the cycle performance of the high-nickel anode material to be measured is qualitatively judged through H2-H3 peak values on the basis of a dQ/dV-curve of capacity increment. The specific principle is as follows: the high nickel cathode material (Ni content more than 80%) is delithiated during charging, and the delithiated amount is gradually increased along with the charging. During the lithium removing process, the following transformation occurs to the crystal phase of the high-nickel cathode material: hexagonal phase H1 → monoclinic phase M → hexagonal phase H2 → hexagonal phase H3. Wherein the phase change of hexagonal phase H1 → monoclinic phase M → hexagonal phase H2 is reversible; when the hexagonal phase H3 is transformed from the hexagonal phase H2, partial irreversible shrinkage occurs in the C-axis direction, and Li+Can not be embedded into the original crystal lattice, resulting in the reduction of electrochemical performance. Therefore, the cycle performance of the material is dominated by the phase change of the hexagonal phase H2 to the hexagonal phase H3, so the cycle performance of the high-nickel cathode material can be rapidly evaluated by adopting the qualitative judgment of H2-H3 peak values.
Compared with the prior art, the rapid evaluation method for the cycle performance of the high-nickel cathode material of the lithium ion battery provided by the invention has the following advantages:
the method is simple to operate, and the process is easy to operate; and the evaluation condition is simple and mild, and the evaluation can be carried out in a normal temperature environment without complex conditions.
The method does not need to carry out full filling for a long time, can greatly reduce energy consumption, saves manpower and material resources, and reduces the evaluation cost of the cycle performance of the high-nickel cathode material. Compared with the traditional method of fully filling and placing till 80% of the initial life, the method shortens the testing time by 40% -70%. The method qualitatively determines the cycle performance of the high-nickel anode material to be measured through the peak values of H2-H3, has strong reliability and wide applicability, can be suitable for button batteries, round batteries, square batteries, soft package batteries and the like, has no limitation on the size of the battery, and can be widely applied to the evaluation of the high-nickel anode material produced in scale.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
FIG. 1 is a dQ/dV-V graph before and after the cycle after steps S02, S03 according to an embodiment of the present invention;
FIG. 2 is a dQ/dV-V graph of three tested high nickel positive electrodes of standard samples QS and A, B, C according to an embodiment of the invention;
fig. 3 is a graph showing the results of three high nickel cathode capacity retention rates to be measured, namely QS and A, B, C, which are standard samples provided by the embodiments of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a method for rapidly evaluating the cycle performance of a high-nickel anode material of a lithium ion battery, which comprises the following steps:
s01, providing a high-nickel anode material to be measured and a standard high-nickel anode material meeting the requirement of preset cycle performance, and respectively assembling the standard high-nickel anode material and the high-nickel anode material to be measured with the same cathode and diaphragm into a battery according to the same method to obtain a standard battery and a battery to be measured; the Ni content in the high-nickel anode material to be measured and the standard high-nickel anode material is not lower than 80%, and the standard battery is marked as QSThe battery to be tested is QX；
S02, performing pre-charging aging and capacity grading treatment on the standard battery and the battery to be tested under the same condition, and performing 0.01-1C charging and discharging circulation on the standard battery and the battery to be tested after capacity grading on a battery detection system, wherein the charging and discharging circulation method comprises the following steps:
charging system: charging to 4.2V at constant current and constant pressure of 0.01-0.1 ℃; standing for 1-30 min;
discharge system: 0.01-0.1C, placing the mixture to 2.75V, and standing for 1-30 min;
s03, collecting data of charging and discharging capacity Q and voltage V, and drawing dQ/dV-V curves of a standard battery and a battery to be tested;
s04, extracting H2-H3 peak values with voltage in a range of 4.0-4.2V according to the dQ/dV-V curve; judging the cycle performance of the standard battery and the battery to be tested according to the H2-H3 peak values and the changes of the standard battery and the battery to be tested; wherein the peak values of the standard battery in the range of 4.0-4.2V from H2-H3 are marked as QS(H2-H3), and the peak values of the to-be-tested battery in the range of 4.0-4.2V, namely H2-H3, are marked as Qx(H2～H3)；
If QX(H2～H3)＞QS(H2-H3), the cycle performance of the high nickel cathode material to be measured is lower than the cycle performance of the standard high nickel cathode material;
if QX(H2～H3)<QS(H2-H3), the cycle performance of the high nickel positive electrode material to be measured is superior to that of the standard high nickel positive electrode material;
if QX(H2～H3)＝QS(H2-H3), and QXThe peak values of H2-H3 are shifted to the right, and the irreversible phase change is increased, so that the cyclicity of the high-nickel anode material to be measured is lower than the cyclicity of the standard high-nickel anode material.
According to the rapid evaluation method for the cycle performance of the high-nickel anode material of the lithium ion battery, provided by the embodiment of the invention, the standard high-nickel anode material meeting the requirement of the preset cycle performance is taken as a reference standard, and the cycle performance of the high-nickel anode material to be measured is qualitatively judged through H2-H3 peak values based on a dQ/dV-V curve of capacity increment. The specific principle is as follows: the high nickel cathode material (Ni content more than 80%) is delithiated during charging, and the delithiated amount is gradually increased along with the charging. During the lithium removing process, the following transformation occurs to the crystal phase of the high-nickel cathode material: hexagonal phase H1 → monoclinic phase M → hexagonal phase H2 → hexagonal phase H3. Wherein the phase change of hexagonal phase H1 → monoclinic phase M → hexagonal phase H2 is reversible; from sixWhen the hexagonal phase H3 is transformed from the cubic phase H2, partial irreversible shrinkage occurs in the C-axis direction, and Li+Can not be embedded into the original crystal lattice, resulting in the reduction of electrochemical performance. Therefore, the cycle performance of the material is dominated by the phase change of the hexagonal phase H2 to the hexagonal phase H3, so the cycle performance of the high-nickel cathode material can be rapidly evaluated by adopting the qualitative judgment of H2-H3 peak values.
Compared with the prior art, the rapid evaluation method for the cycle performance of the high-nickel cathode material of the lithium ion battery provided by the embodiment of the invention has the following advantages:
the method is simple to operate, and the process is easy to operate; and the evaluation condition is simple and mild, and the evaluation can be carried out in a normal temperature environment without complex conditions.
The method does not need to carry out full filling for a long time, can greatly reduce energy consumption, saves manpower and material resources, and reduces the evaluation cost of the cycle performance of the high-nickel cathode material. Compared with the traditional method of fully filling and placing till 80% of the initial life, the method shortens the testing time by 40% -70%.
The method qualitatively determines the cycle performance of the high-nickel anode material to be measured through the peak values of H2-H3, has strong reliability and wide applicability, can be suitable for round batteries, square batteries, soft package batteries and the like, has no limitation on the size of the batteries, and can be widely applied to the evaluation of the high-nickel anode material produced in scale.
Specifically, in step S01, a high nickel cathode material to be measured is provided, and the high nickel cathode material to be measured may be a high nickel cathode material of any battery type and any battery size. For example, the high-nickel positive electrode material to be measured may be a high-nickel positive electrode material for a button cell battery, may be a high-nickel positive electrode material for a cylindrical battery, may also be a high-nickel positive electrode material for a soft package battery, and may also be a high-nickel positive electrode material for a square battery.
Providing a standard high-nickel anode material meeting the preset cycle performance requirement, wherein the standard high-nickel anode material meeting the preset cycle performance requirement refers to a standard high-nickel anode material meeting a certain preset cycle requirement. Likewise, the standard high nickel positive electrode material can be a high nickel positive electrode material of any battery model and any battery size. For example, the standard high-nickel positive electrode material may be a high-nickel positive electrode material for a button cell battery, a high-nickel positive electrode material for a cylindrical battery, a high-nickel positive electrode material for a soft package battery, or a high-nickel positive electrode material for a square battery.
The preset cycle performance requirement of the standard high-nickel anode material is set according to the actual application requirement of the high-nickel anode material to be measured. Preferably, the standard high-nickel cathode material is a high-nickel cathode material with cycle efficiency of more than 80% after 1000 cycles. In some embodiments, the standard high nickel positive electrode material is a high nickel positive electrode material having a cycle efficiency of 80% after 1000 cycles; in some embodiments, the standard high nickel positive electrode material is a high nickel positive electrode material with a cycle efficiency of 82% after 1000 cycles; in some embodiments, the standard high nickel positive electrode material is a high nickel positive electrode material with a cycle efficiency of 85% after 1000 cycles; in some embodiments, the standard high nickel positive electrode material is a high nickel positive electrode material with a cycle efficiency of 88% after 1000 cycles; in some embodiments, the standard high nickel positive electrode material is a high nickel positive electrode material with a cycle efficiency of 90% after 1000 cycles; in some embodiments, the standard high nickel positive electrode material is a high nickel positive electrode material with a cycle efficiency of 92% after 1000 cycles; in some embodiments, the standard high nickel cathode material is a high nickel cathode material with a cycle efficiency of 95% after 1000 cycles.
It should be noted that, in the embodiment of the present invention, the high nickel positive electrode material (including the high nickel positive electrode material to be measured and the standard high nickel positive electrode material) refers to a nickel-containing positive electrode material in which the weight percentage of nickel element in the positive electrode material is higher than 80% (may be 80%). Specifically, in the standard high-nickel cathode material, the weight percentage of nickel element accounts for more than 80% of the total weight of the cathode material; in the nickel anode material to be measured, the weight percentage of nickel element accounts for more than 80% of the total weight of the anode material. When the nickel content of the high-nickel cathode material is lower than 80%, the rapid evaluation provided by the embodiment of the invention is not applicable to judging the cycle performance of the high-nickel cathode material of the lithium ion battery.
The closer the nickel element content in the standard high-nickel anode material and the high-nickel anode material to be measured is, the stronger the comparability of the cycle performance of the high-nickel anode material determined by the method is, and the more accurate the evaluation result is. In some embodiments, the weight percentage of nickel element in the standard high nickel positive electrode material and the weight percentage of nickel element in the high nickel positive electrode material to be measured differ by less than 5%. In some embodiments, the weight percentage content of the nickel element in the standard high-nickel cathode material is the same as the weight percentage content of the nickel element in the high-nickel cathode material to be measured, and the evaluation of the cycle performance of the high-nickel cathode material to be measured is most accurate.
In the embodiment of the invention, the high nickel anode material to be measured and the standard high nickel anode material have the same element components, and the high nickel anode material to be measured and the standard high nickel anode material have comparability. In some embodiments, the positive electrode material of the high nickel positive electrode material to be measured and the standard high nickel positive electrode material is NCM811 (lithium nickel cobalt manganese oxide: LiNi)0.8Co0.1Mn0.1O2) (ii) a In some embodiments, the positive electrode material of the high nickel positive electrode material to be measured and the standard high nickel positive electrode material is NCA (nickel cobalt lithium aluminate: LiNi)0.8Co0.15Al0.05O2)。
And respectively assembling the provided standard high-nickel anode material and the high-nickel anode material to be measured with the same cathode and the same diaphragm into a battery according to the same method to obtain the standard battery and the battery to be measured. Except for the difference of the high-nickel anode material, other components and parts forming the assembled battery and the preparation method thereof are completely consistent so as to eliminate the influence of other factors on the cycle performance evaluation of the high-nickel anode material. For convenience of the following description, the standard cell is labeled QSThe battery to be tested is QX。
In some embodiments, the negative electrode is selected from a lithium negative electrode or a graphite negative electrode, but the negative electrode materials of the standard battery and the battery to be tested are the same. In some embodiments, in the step of assembling the standard high-nickel positive electrode material and the high-nickel positive electrode material to be measured with the same negative electrode and the same separator into the battery respectively according to the same method, the battery is one of a button battery, a cylindrical battery, a soft package battery and a square battery, but the standard battery and the battery to be measured have the same battery type.
In the step S02, the standard battery and the battery to be tested are subjected to pre-charge aging and capacity grading under the same condition, which may be performed by a conventional method, and only the method, parameters, conditions, and the like of the pre-charge aging and capacity grading of the standard battery and the battery to be tested need to be satisfied to be completely consistent.
Furthermore, the standard battery and the battery to be detected after capacity grading are taken to be subjected to charge-discharge circulation of 0.01C-1C on a battery detection system, and the method for single charge-discharge circulation comprises the following steps:
charging system: charging to 4.2V at constant current and constant pressure of 0.01-0.1 ℃; standing for 1-30 min;
discharge system: 0.01-0.1C, placing the mixture to 2.75V, and standing for 1-30 min.
In some embodiments, the standard battery and the battery to be tested after capacity grading are taken to be subjected to charge and discharge circulation at 0.01C-1C on the battery detection system, and the method of the single charge and discharge circulation is as follows:
charging system: charging to 4.2V at constant current and constant pressure of 0.01-0.5 ℃; standing for 5 min;
discharge system: 0.01-0.5C, 2.75V, and standing for 5 min.
And (3) carrying out charge-discharge circulation under the conditions, wherein the high-nickel cathode material has the following crystal phase transformation in the charging process: hexagonal phase H1 → monoclinic phase M → hexagonal phase H2 → hexagonal phase H3. Furthermore, the cycle performance of the high-nickel cathode material can be rapidly evaluated through irreversible transformation from hexagonal phase H2 to hexagonal phase H3.
In some embodiments, charge and discharge cycles are performed between 1 and 5 times to eliminate the effects of cell instability factors, such as SEI and CEI reformation and active lithium depletion by repair.
In step S03, data of the charge and discharge capacity (Q) and the voltage (V) are collected, dQ/dV-V curves of the standard battery and the battery to be tested are drawn, and when the charge and discharge cycle is more than one time, data of the capacity (Q) and the voltage (V) of the last charge and discharge cycle are preferentially selected and collected, and the dQ/dV-V curves of the charge and discharge cycles of the standard battery and the battery to be tested are drawn.
FIG. 1 shows graphs of dQ/dV-V before and after the cycle after steps S02 and S03.
In the step S04, according to the dQ/dV-V curve, H2 to H3 peaks of a voltage range of 4.0 to 4.2V are extracted, that is, phase transition position voltage range data of the hexagonal phase H2 to the hexagonal phase H3 is extracted. And judging the cycle performance of the standard battery and the battery to be tested according to the H2-H3 peak values of the standard battery and the battery to be tested and the displacement change of the battery to be tested relative to the H2-H3 peak values of the standard battery and the battery to be tested. In particular, the method comprises the following steps of,
if QX(H2～H3)＞QS(H2-H3), the cycle performance of the high nickel cathode material to be measured is lower than the cycle performance of the standard high nickel cathode material;
if QX(H2～H3)<QS(H2-H3), the cycle performance of the high nickel positive electrode material to be measured is superior to that of the standard high nickel positive electrode material;
if QX(H2～H3)＝QS(H2-H3), and QXThe peak values of H2-H3 are shifted to the right, and the irreversible phase change is increased, so that the cyclicity of the high-nickel anode material to be measured is lower than the cyclicity of the standard high-nickel anode material.
Therefore, the cycle performance of the high-nickel anode material to be tested (relative to the standard high-nickel anode material) can be rapidly evaluated through analyzing the H2-H3 peak values of the standard battery and the battery to be tested and the displacement change of the battery to be tested relative to the H2-H3 peak values of the standard battery and the battery to be tested.
According to the rapid evaluation method for the cycle performance of the high-nickel anode material of the lithium ion battery, provided by the embodiment of the invention, when the high-nickel anode material of the lithium ion battery is selected, Qs is taken as a standard, and the positions of H2-H3 peaks of a Qx capacity increment dQ/dV-V curve are qualitatively judged, so that a supplier material with better cycle performance can be screened.
In some embodiments, after the step of determining the cycle performance of the standard battery and the battery to be tested, the method further includes: and carrying out SOC local accelerated circulation on the standard battery and the battery to be tested in the same standard, and judging the cycle performance of the high-nickel anode material to be tested in the battery to be tested according to the result of the SOC local accelerated circulation. Because the SOC interval just comprises the phase change interval from H2 to H3, the cycle performance of the high-nickel anode material to be measured (relative to a standard high-nickel anode material) is further quantitatively judged by combining a local SOC cycle method based on a dQ/dV-V curve of the capacity increment, and the cycle performance of the high-nickel anode material is rapidly evaluated.
In the embodiment of the present invention, the SOC is called State of Charge, and represents a ratio of a remaining capacity of the battery after being used for a certain period of time or left unused for a long time to a capacity of a fully charged State thereof, and is expressed by a common percentage. The value range is 0-100%, when SOC is 0, the battery is completely discharged, and when SOC is 100%, the battery is completely full. The method of local SOC circulation is a method of selecting a proper local electric quantity range between 0-100% electric quantity to carry out circulation test. The local charge difference Δ SOC is the difference between the high SOC and the low SOC of the battery.
In some embodiments, the method of SOC local acceleration cycling is: charging and discharging at 0.2-1C, discharging the battery to 2.75V, charging to a first cut-off voltage marker SOC1, and then discharging to a second cut-off voltage marker SOC2 to form a charge-discharge cycle; and repeating the charge-discharge cycle for more than 50 times, performing full charge-discharge test on the capacity retention rate, comparing the capacity retention rates of the standard battery and the battery to be tested, and judging the cycle performance of the high-nickel anode material to be tested, so that the cycle performance of the high-nickel anode material to be tested can be evaluated more quickly.
In some embodiments, the state difference between the SOC1 corresponding to the first cut-off voltage and the SOC2 corresponding to the second cut-off voltage is labeled as Δ SOC, which must include the phase transition region H2-H3, and the Δ SOC is 20% to 50%. If the delta SOC is too large, the evaluation time is too long, and the full charge and discharge tend to be realized by the traditional method; if the delta SOC is too small, the phase change interval from H2 to H3 cannot be truly reflected, and the accuracy of the evaluation result is not high.
In some embodiments, the SOC local acceleration cycling profile is: the current charge and discharge are carried out at 0.2C-1C, and the electric quantity difference delta SOC is between 20 and 50 percent; the SOC cycle is controlled by time, the battery is discharged to 2.75V, then the battery is charged to the cut-off capacity (the charge cut-off capacity is 100%) by the charge time, the battery is discharged to the cut-off capacity (the discharge cut-off capacity ranges from 50% to 80%) by the discharge time, and then the cycle test is carried out between the charge cut-off capacity and the discharge cut-off capacity.
In some embodiments, the first cut-off charge amount is 100%, that is, the charge-discharge cycle of the SOC local acceleration cycle is charged until the charge-cut-off charge amount of 100% is reached; in some embodiments, the second cut-off charge amount is 50% to 80%, that is, in the charge and discharge cycle of the SOC local acceleration cycle, the discharge is performed until 50% to 80% of the discharge cut-off charge amount is reached. In some embodiments, the first off charge is 100% and the second off charge is 50% to 80%.
In some embodiments, the number of the charge and discharge cycles is 500 to 50000 times, and specifically may be 500 times, 700 times, 1000 times, 2000 times, 3000 times, 4000 times, 5000 times, 8000 times, 10000 times, 20000 times, 30000 times, 40000 times, 50000 times.
Taking Δ SOC of 40% as an example, the SOC is controlled with time, the cycle is performed in the SOC range of 60-100%, the charge cut-off SOC of 100% and the discharge cut-off SOC of 60%, the above steps S02 and S03 are repeated after 1000 cycles, the capacity after 1000 cycles is determined, and the capacity retention rate after 1000 cycles is calculated. The lowest SOC is 0 and the highest SOC is 100%.
In some embodiments, the Δ SOC is 40%, and the SOC electric quantity interval is selected from 60% to 100%, that is, the first cut-off electric quantity is 100%, and the second cut-off electric quantity is 60%, at this time, the charge-discharge cycle process includes a phase change interval from H2 to H3, so that the cycle performance of the high-nickel cathode material of the lithium ion battery can be evaluated more accurately.
According to the embodiment of the invention, the circulation performances of the standard high-nickel material battery and the high-nickel material battery to be tested are qualitatively screened and judged through the peak values of the dQ/dV-V curves H2-H3, and the material to be tested with the circulation performance superior to that of the standard high-nickel material or the material to be tested with the circulation performance equivalent to that of the standard high-nickel material is preliminarily screened out. Furthermore, the screened material is fully filled and discharged through 50-50000 local accelerated cycles and 2-5 cycles, and the capacity retention rate after the cycles can be determined.
The following description will be given with reference to specific examples.
The apparatus used in the following examples: electrochemical workstation, battery test arbin device.
Example 1
A rapid evaluation method for cycle performance of a high-nickel cathode material of a lithium ion battery comprises the following steps:
s11, providing a high-nickel anode material to be measured and a standard high-nickel anode material meeting the requirement of preset cycle performance, and respectively assembling the standard high-nickel anode material and the high-nickel anode material to be measured with the same cathode and diaphragm into a cylindrical 18650 battery according to the same method to obtain a standard battery and a battery to be measured; the high-nickel anode material to be measured and the standard high-nickel anode material are the same, and the weight percentage of nickel element in the standard high-nickel anode material accounts for more than 80% of the total weight of the anode material; in the nickel anode material to be measured, the weight percentage of nickel element accounts for more than 80% of the total weight of the anode material; the standard battery is marked as QSThe battery to be tested is QX；
And S12, performing pre-charging aging and grading treatment on the standard battery and the battery to be tested by a conventional process. The batteries after capacity grading are taken out and charged and discharged for 3 cycles on a battery arbin test cabinet at 0.05C:
charging system: charging to 4.2V at constant current and constant voltage of 0.05 ℃; standing for 5 min;
discharge system: cooling to 2.75V at 0.05C, and standing for 5 min;
s13, taking the discharge capacity of the last cycle as the standard capacity, and carrying out differential processing on the data of the charge curve and the discharge curve of the last cycle by using data processing software to make a standard sample QSAnd a sample Q to be measuredXThe dQ/dV-V curve of (1); according to the H2-H3 peak values and the variation of the standard battery and the battery to be testedConverting, namely judging the cycle performance of the standard battery and the battery to be tested;
s14, SOC local acceleration circulation: charging and discharging with 1C current, wherein delta SOC is 40%, SOC electric quantity range is 60% to 100% SOC, the battery is discharged to 2.75V in the first step, the battery is charged to 100% SOC by time control in the second step, charging time is 60min, discharging is controlled to 60% electric quantity by time control in the third step, discharging time is 24min, rest is 10min, the battery is recharged to 100% SOC in the fourth step, charging time is 24min, and the third step and the fourth step are a cycle; cycling 500 times between 60% and 100% SOC;
and comparing the results of the step S13 and the step S14, and performing comparative analysis to obtain a test result, namely, quickly evaluating the cycle performance of the high-nickel cathode material.
Standard high-nickel cathode material Q prepared by the method of example 1SA, B, C evaluation is carried out on the three high nickel anode materials to be measured, and the dQ/dV-V curves before and after the circulation after the steps S12 and S13 are shown in FIG. 2. As can be seen from fig. 2:
and judging the cycle performance of the standard high-nickel anode material and the high-nickel anode material to be detected according to the peak values and peak shifts of H2-H3. Compared with the peak values H2-H3 of the standard high-nickel positive electrode material QS:
A＞QSthe A cycle performance is presumed to be inferior to the QS standard sample;
C＜QSthe C cycle performance is presumed to be superior to the standard QS.
B and C have the same H2-H3 peak values, wherein the H2-H3 peak values of B shift to the right, irreversible phase change is increased, and B cycle performance is supposed to be inferior to C.
Therefore, the high nickel anode material C, the pair C and the pair Q to be measured can be preferably selectedSFurther evaluating the local 60% -100% SOC accelerated cycle: the first step is full charge and discharge (0-100% SOC) to determine the discharge capacity, after 700 circles of accelerated cycles, the second full charge and discharge (0-100% SOC) to determine the discharge capacity, and the ratio of the two discharge capacities before and after the first step is the capacity retention rate after 700 circles. The evaluation results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the capacity retention of C is greater than that of Q after 700 acceleration cyclesSThe height is 2.8 percent.
To compare the correctness of the data, fig. 3 directly shows a standard high nickel cathode material QSAnd A, B, C, namely A, B, C, three samples to be tested, namely the high nickel anode capacity retention rate to be tested (wherein the abscissa Cyc.Num represents the cycle number, and the ordinate Cap.ret represents the capacity retention rate).
Similarly, the results show that the C cycle is better, and the capacity maintenance after 700 cycles is 2.6% higher than QS, which are comparable in test results. The local acceleration cycle retention rate of the 60-100% SOC is higher than that of the 0-100% SOC, and the phase change of the hexagonal phase H1 → the monoclinic phase M → the hexagonal phase H2 cannot be comprehensively monitored due to the 60-100% SOC, and only the phase change of H2 → H3 is considered and monitored; although H1 → M → H2 is reversible, the stress and polarization caused by multiple phase transitions in the actual 0-100% SOC cycle process are increased compared with the 60-100% SOC cycle, so the retention rate of the 0-100% SOC cycle is low.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A method for rapidly evaluating the cycle performance of a high-nickel cathode material of a lithium ion battery is characterized by comprising the following steps of:
providing a high-nickel anode material to be measured and a standard high-nickel anode material meeting the preset cycle performance requirement, and respectively assembling the standard high-nickel anode material and the high-nickel anode material to be measured with the same cathode and diaphragm into a battery according to the same method to obtain a standard battery and a battery to be measured; the Ni content in the high-nickel anode material to be measured and the standard high-nickel anode material is not lower than 80%, and the standard battery is marked as QSThe battery to be tested is QX；
Performing pre-charging aging and capacity grading treatment on the standard battery and the battery to be tested under the same condition, and performing 0.01-1C charging and discharging circulation on the standard battery and the battery to be tested after capacity grading on a battery detection system, wherein the circulation method comprises the following steps:
charging system: charging to 4.2V at constant current and constant pressure of 0.01-0.1 ℃; standing for 1-30 min;
discharge system: 0.01-0.1C, placing the mixture to 2.75V, and standing for 1-30 min;
collecting data of charging and discharging capacity Q and voltage V, and drawing dQ/dV-V curves of a standard battery and a battery to be tested;
extracting H2-H3 peak values with the voltage of 4.0-4.2V according to the dQ/dV-V curve; judging the cycle performance of the standard battery and the battery to be tested according to the H2-H3 peak values and the changes of the standard battery and the battery to be tested; wherein the peak values of the standard battery in the range of 4.0-4.2V from H2-H3 are marked as QS(H2-H3), and the peak values of the to-be-tested battery in the range of 4.0-4.2V, namely H2-H3, are marked as Qx(H2～H3)；
If QX(H2～H3)＞QS(H2-H3), the cycle performance of the high nickel cathode material to be measured is lower than the cycle performance of the standard high nickel cathode material;
if QX(H2～H3)<QS(H2-H3), the cycle performance of the high nickel positive electrode material to be measured is superior to that of the standard high nickel positive electrode material;
if QX(H2～H3)＝QS(H2-H3), and QXThe peak values of H2-H3 are shifted to the right, and the irreversible phase change is increased, so that the cyclicity of the high-nickel anode material to be measured is lower than the cyclicity of the standard high-nickel anode material.
2. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery according to claim 1, wherein after the step of judging the cycle performance of the standard battery and the battery to be tested, the method further comprises the following steps: and carrying out SOC local accelerated circulation on the standard battery and the battery to be tested in the same standard, and judging the cycle performance of the high-nickel anode material to be tested in the battery to be tested according to the result of the SOC local accelerated circulation.
3. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery according to claim 2, wherein the method for locally accelerating the cycle of the SOC comprises the following steps: charging and discharging at 0.2-1C, discharging the battery to 2.75V, charging to a first cut-off voltage, and then discharging to a second cut-off voltage to form a charge-discharge cycle; and repeating the charge-discharge cycle for more than 50 times, carrying out full charge-discharge test on the capacity retention rate, comparing the capacity retention rates of the standard battery and the battery to be tested, and judging the cycle performance of the high-nickel anode material to be tested.
4. The method for rapidly evaluating the cycle performance of the lithium ion battery high-nickel cathode material according to claim 3, wherein the first cut-off voltage is labeled as SOC1, the second cut-off voltage is labeled as SOC2, and the difference between the SOC1 and the SOC2 is labeled as Δ SOC, and the Δ SOC is 20% to 50%, wherein the SOC represents the state of charge or the remaining charge, and the Δ SOC represents the local charge difference.
5. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery as claimed in claim 4, wherein the first cut-off voltage SOC1 is 100%; and/or
The second cut-off voltage SOC2 is 50% -80%; and/or
The number of the charging and discharging cycles is 1000-50000.
6. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery according to any one of claims 1 to 5, wherein the weight percentage of nickel element in the standard high-nickel cathode material accounts for more than 80% of the total weight of the cathode material; in the nickel anode material to be measured, the weight percentage of nickel element accounts for more than 80% of the total weight of the anode material.
7. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery as claimed in claim 6, wherein the weight percentage of the nickel element in the standard high-nickel cathode material and the weight percentage of the nickel element in the high-nickel cathode material to be measured are different by less than 5%.
8. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery according to claim 7, wherein the weight percentage of the nickel element in the standard high-nickel cathode material is the same as the weight percentage of the nickel element in the high-nickel cathode material to be measured.
9. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery according to any one of claims 1 to 5, wherein the standard high-nickel cathode material is a high-nickel cathode material with a cycle efficiency of more than 80% after 1000 cycles.
10. The method for rapidly evaluating the cycle performance of the high-nickel cathode material of the lithium ion battery according to any one of claims 1 to 4, wherein the cathode material in the high-nickel cathode material to be measured and the standard high-nickel cathode material is NCM 811; and/or
The negative electrode is selected from a lithium negative electrode or a graphite negative electrode or a silicon-containing negative electrode; and/or
And respectively assembling the standard high-nickel positive electrode material and the high-nickel positive electrode material to be measured with the same negative electrode and the same diaphragm into a battery according to the same method, wherein the battery is one of a button battery, a cylindrical battery, a soft package battery and a square battery.
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| CN111551572B (en) * | 2020-05-21 | 2023-02-03 | 安徽科达新材料有限公司 | Method for rapidly evaluating cycle performance of graphite material in battery |
| CN112363069B (en) * | 2020-09-18 | 2023-07-07 | 万向一二三股份公司 | Method for detecting breakage of tab of lithium ion battery |
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| CN112834944B (en) * | 2020-12-30 | 2023-03-07 | 上海兰钧新能源科技有限公司 | Lithium battery accelerated cycle life testing method, device, medium and equipment |
| CN113659214B (en) * | 2021-07-12 | 2023-03-17 | 深圳市比克动力电池有限公司 | Design method of high specific energy lithium ion battery with electrochemical performance and safety performance |
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